KR101584120B1 - Manufacturing method of pure nickel sulfate from leaching residue being removed cobalt of lithium secondary battery - Google Patents
Manufacturing method of pure nickel sulfate from leaching residue being removed cobalt of lithium secondary battery Download PDFInfo
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- KR101584120B1 KR101584120B1 KR1020150071491A KR20150071491A KR101584120B1 KR 101584120 B1 KR101584120 B1 KR 101584120B1 KR 1020150071491 A KR1020150071491 A KR 1020150071491A KR 20150071491 A KR20150071491 A KR 20150071491A KR 101584120 B1 KR101584120 B1 KR 101584120B1
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- nickel
- secondary battery
- nickel sulfate
- lithium secondary
- cobalt
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
Abstract
More particularly, the present invention relates to a method for producing high purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery, and more particularly, to a method for producing high purity nickel sulfate from a lithium secondary battery, ; Mixing the nickel-extracted organic phase with a stripping agent to concentrate the nickel; And crystallizing the concentrated nickel by heating and then cooling the nickel. The present invention also relates to a method for producing high purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery.
Description
The present invention relates to a method for producing high purity nickel sulfate from a solution obtained by extracting cobalt from a cathode active material of a lithium secondary battery.
Lithium secondary batteries are expected to increase rapidly in applications for hybrid vehicles. Manganese, cobalt, nickel, lithium and the like are used as a cathode active material of such a lithium ion battery. As the amount of waste lithium secondary battery generated increases, attention is focused on a recovery method in terms of resource recycling. In the case of lithium secondary batteries, LCO (LiCoO 2 ) system, which is mainly composed of lithium and cobalt, was mainly used. However, in order to replace expensive cobalt, NCM (NiCoMn) system containing a lot of nickel and manganese A process for separating and recovering cobalt, nickel and lithium at the same time is required to be developed.
In the wet process for recovering the valuable metal from the cathode active material of lithium secondary battery, the pretreated sample is first leached with a metal component such as cobalt using sulfuric acid, and then the metal such as iron, aluminum, The components are precipitated off by adjusting the pH. Thereafter, the manganese in the solution is removed by solvent extraction or KMnO 4 , and the solution mainly contains the three components of cobalt, nickel and lithium. In this solution, cobalt can be selectively separated from nickel and lithium ions using an extractant to recover cobalt. On the other hand, nickel and lithium and sodium are present in the remaining extraction residue after extraction and separation of cobalt. When nickel is separated from this solution by using an extracting agent, a large amount of nickel is present in the extractive filtrate and a large amount of impurities are contained. There is a problem that nickel sulfate can not be manufactured.
As a prior art related thereto, there is a method of recovering valuable metal from the cathode material of a spent lithium ion battery disclosed in Korean Patent Laid-Open Publication No. 10-2014-0126943 (published on April 11, 2014).
Accordingly, it is an object of the present invention to provide a method for producing nickel sulfate of high purity by extracting nickel from an extraction residue left after cobalt extraction in a cathode active material of a lithium secondary battery.
The problems to be solved by the present invention are not limited to the above-mentioned problem (s), and another problem (s) not mentioned can be understood by those skilled in the art from the following description.
In order to solve the above-mentioned problems, the present invention provides a method for producing nickel, comprising: extracting cobalt from a cathode active material of a lithium secondary battery; Mixing the nickel-extracted organic phase with a stripping agent to concentrate the nickel; And crystallizing the concentrated nickel by heating and then cooling it to provide a high purity nickel sulfate from the cobalt extraction residue of the lithium secondary battery.
According to the present invention, the extraction agent is mixed with a basic solution and saponified at 60% by volume or more to extract cobalt from the cathode active material of the lithium secondary battery, and then nickel is easily extracted into the organic phase from the remaining extraction residue. Most of the nickel can be extracted into the organic phase.
Also, most of the nickel present in the extraction residue can be extracted into the organic phase by performing the step of extracting nickel into the organic phase in four stages, thereby producing nickel sulfate having a purity of 99.99%.
1 is a flowchart showing a method for producing nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention.
FIG. 2 is a photograph of nickel sulfate manufactured by a method for producing nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention.
FIG. 3 is a graph showing the extraction ratio of the extractant according to the saponification in the nickel sulfate production process from the cobalt extraction residue of the lithium secondary battery according to the present invention.
4 is a graph showing a cleaning rate according to the concentration of sulfuric acid in a production method of nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention.
5 is a graph showing a cleaning rate according to the concentration of sulfuric acid in the production method of nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention.
FIG. 6 is a graph showing removal rates according to sulfuric acid concentration in the production process of nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention. FIG.
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS The advantages and features of the present invention and the manner of achieving it will become apparent with reference to the embodiments described in detail below with reference to the accompanying drawings.
The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. To fully disclose the scope of the invention to those skilled in the art, and the invention is only defined by the scope of the claims.
In the following description, well-known functions or constructions are not described in detail since they would obscure the invention in unnecessary detail.
The present invention relates to a method for preparing a lithium secondary battery, comprising the steps of: extracting cobalt from a cathode active material of lithium secondary battery and then mixing the remaining extraction liquid with an extractant and a basic solution to extract nickel as an organic phase;
Mixing the nickel-extracted organic phase with a stripping agent to concentrate the nickel; And
And heating and crystallizing the concentrated nickel. The present invention also provides a method for producing high purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery.
The method for producing high purity nickel sulfate from the cobalt extraction residue of the lithium secondary battery according to the present invention comprises extracting cobalt from the lithium secondary battery cathode active material by mixing the extracting agent with a basic solution and saponifying the mixture at not less than 60 vol% Nickel in the organic phase can be easily extracted and most of the nickel present in the extraction residue can be extracted into the organic phase. Also, most of the nickel present in the extraction residue can be extracted into the organic phase by performing the step of extracting nickel into the organic phase in four stages, thereby producing nickel sulfate having a purity of 99.99%.
1 is a flowchart showing a method for producing high purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention. Hereinafter, the present invention will be described in detail with reference to Fig.
The method for producing high-purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention comprises the steps of: extracting cobalt from a cathode active material of a lithium secondary battery and then mixing the remaining extraction liquid with an extractant and a basic solution to extract nickel into an organic phase S10).
In the method for producing high purity nickel sulfate from the cobalt extraction residue of the lithium secondary battery according to the present invention, the lithium ion battery includes manganese, cobalt, nickel, lithium and sodium, and is used for separation and recovery of cobalt, nickel, The extraction process is performed, and the extraction residue in the present invention is the solution remaining after extracting cobalt from the lithium ion battery. At this time, the extraction residue remaining after extracting the cobalt contains 10 to 12 g / L of Ni, 4 to 5 g / L of Li and 2 to 3 g / L of Na.
The extractant may be selected from the group consisting of di-2-ethylhexylphosphoric acid (D2EHPA), 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester, ethylhexyl ester: PC88A), a mixture of di-2-ethylhexylphosphoric acid and tri-butyl-phosphate (TBP) and a mixture of 2-ethylhexylphosphonic acid mono- A mixture of 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester and tri-butyl-phosphate (TBP) may be used.
Also, the basic solution may be NaOH or NH 4 OH, and the basic solution preferably has a concentration of 15 to 25% by volume. When the concentration of the basic solution is less than 15% by volume, there is a problem that the extraction efficiency of nickel is lowered due to the low equilibrium pH. When the concentration exceeds 25% by volume, a solid is formed due to saponification, There is a problem in that impurities of the above-mentioned impurities are extracted.
The basic solution is preferably mixed at a volume ratio of 0.1 to 0.2 based on the extracting agent. When the basic solution is mixed at less than 0.1 part by volume with respect to the extracting agent, the saponification of the extracting agent is less than 60% by volume, and the concentration of nickel in the organic phase is lowered. On the other hand, when the basic solution is more than 0.2 part by volume, There is a problem that the purity of the nickel sulfate produced by including a metal such as lithium in the organic phase is lowered.
In addition, the ratio of the organic phase / water phase (O / A) in the mixture of the extraction residue remaining after extracting the cobalt with the extractant and the basic solution is preferably 1. When the ratio of the organic phase / water phase is other than 1, the boundary between the organic phase and the water phase is not clear, so that only the organic phase can not be obtained and the concentration of lithium in the organic phase increases.
Also, the ratio of the organic phase to the aqueous phase (O / A) in the mixture of the extraction residue remaining after extracting the cobalt and the extractant and the basic solution can vary from 1 to 10, but the case of 1 is suitable for the process operation.
The extraction step is preferably performed four times. When the extraction process is carried out three times or less, there is a problem that nickel is not completely extracted and a large amount of nickel is present in the aqueous phase. In the case where the extraction process is performed more than four times, It is preferable to perform it four times.
Next, a method for producing high-purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention includes a step (S20) of mixing the organic phase from which the nickel is extracted with a detaching agent to concentrate lithium.
The removing agent may be sulfuric acid, and the concentration of the removing agent is preferably 4 to 6 M. When the concentration of the removing agent is less than 4M, the removal rate of lithium in the organic phase is lowered and the impurities remain. In the case of exceeding 6M, the pH of the removing solution is lowered, It is preferable that the thickness is 6M or less.
The method for producing high-purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention includes a step (S30) of heating the concentrated nickel and then cooling it to crystallize it.
In the process for producing high purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention, the concentrated nickel can be heated at 70 to 90 ° C and then cooled to crystallize into nickel sulfate of NiSO 4 .6H 2 O, Of high-purity nickel sulfate can be produced. If the heating is less than 70 ° C, there is a problem that high-purity nickel sulfate can not be produced. If the heating is above 90 ° C, nickel sulfate of hexahydrate can not be produced and nickel sulfate used for plating and battery precursor production can not be used there is a problem.
The method for producing high purity nickel sulfate from the cobalt extraction residue of the lithium secondary battery according to the present invention may further include a step of washing the nickel-extracted organic phase.
Sulfuric acid may be used as a cleaning agent for cleaning the organic phase, and the concentration of the cleaning agent is preferably 0.2 to 0.4 M. When the concentration of the detergent is less than 0.2M, the effect of removing sodium and lithium is low. When the concentration of the detergent is more than 0.4M, nickel is removed in the organic phase.
Example 1: Preparation of high purity nickel sulfate 1
450 ml of D2EHPA was added to the extraction residue after extracting the cobalt solvent from the leached lithium secondary battery, and 54 ml of 20 vol% NaOH solution was added to saponify D2EHPA to 60% by volume. At this time, the ratio of organic phase / water phase was set to 1, and nickel was extracted as an organic phase.
The extraction balance after extracting the cobalt solvent from the leached lithium secondary battery contained 11.9 g / L of Ni, 4 g / L of Li and 2.7 g / L of Na, and the pH was 6.
4M sulfuric acid was added to the nickel extracted with the organic phase, and the nickel was removed. The concentrated nickel was heated to 80 ° C and then cooled to room temperature to prepare high purity nickel sulfate (see FIG. 2).
Example 2: Preparation of high purity nickel sulfate 2
High purity nickel sulfate was prepared in the same manner as in Example 1 except that nickel was extracted with an organic phase and then washed with 0.4 M sulfuric acid.
Experimental Example 1: Analysis of nickel concentration according to the number of times of extraction in the extraction process
The concentration of nickel according to the number of times of extraction in the extraction process in the process for producing high purity nickel sulfate from the cobalt extraction residue of the lithium secondary battery according to the present invention was analyzed.
During the extraction process, 54 ml of 20 vol% NaOH was added to 450 ml of extractant D2EHPA, where the O / A ratio was 1.
The ICP values of the raffinate at each stage were 11.51 g / L, 5.87 g / L, and 821 ppm, respectively. appear.
In addition, the pH of each step was 4.38, 4.42, 4.70, and 7.68, respectively, in the first stage to the fourth stage. In this case, the concentration of Ni in each raffinate was 11.51 g / L, 7.63 g / L, 2.64 g / L and 176 ppm, respectively.
From the above results, it can be seen that when extracting 4 steps from O / A ratio 1, Ni can be extracted to 98.5%, and it is possible to extract 13 g / L of Ni, 600 ppm of Li and 2.8 g / L of Na An organic phase was obtained.
FIG. 3 is a graph showing extraction behavior of Ni and Li according to saponification of an extractant in a process for producing high purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention. As shown in FIG. 2, as the saponification increased to 50% by volume, the extraction ratio of Ni increased from 41% to 64%, and that of Li increased from 23.9% to 29.38%.
Experimental Example 2: Analysis of cleaning rate of organic phase according to sulfuric acid concentration
The cleaning ratios of the organic phase according to the sulfuric acid concentration in the process for producing high purity nickel sulfate from the cobalt extraction residue of the lithium secondary battery according to the present invention were examined and the results are shown in Tables 1, 4, 2 and 5.
Ni, Li and Na were cleaned from the organic phase containing 13 g / L of Ni, 600 ppm of Li and 2.8 g / L of Na.
Table 1 below shows the cleaning ratios of the organic phase to the concentration of sulfuric acid in the 800 ppm Ni solution.
FIG. 4 is a graph showing a cleaning rate according to sulfuric acid concentration in a process for producing high purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention. FIG.
As shown in Table 1 and FIG. 4, in the case of Na, the removal rate was 66.24% at the removal rate of 36.33% when the sulfuric acid concentration was increased. However, when the concentration of sulfuric acid was increased from 0.2M to 0.4M in the case of Li, 40% increase, indicating that Li is not easily removed but has a cleaning effect.
Table 2 shows the cleaning ratios of the organic phase according to the sulfuric acid concentration in the 8000 ppm Ni solution.
FIG. 5 is a graph showing a cleaning rate according to sulfuric acid concentration in a process for producing high purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention. FIG.
As shown in Table 2 and FIG. 5, in the case of Na, the cleaning rate increased from 49.77% to 68% when the concentration of sulfuric acid was ranged from 0.2M to 0.4M. In the case of Li, the concentration of sulfuric acid was increased from 0.2M to 0.4 M, it showed a 37% to 41% increase, indicating that it was not easily removed but had a cleaning effect.
Experimental Example 3: Analysis of removal rate according to sulfuric acid concentration
The removal rates of the high-purity nickel sulfate from the cobalt extraction residue of the lithium secondary battery according to the present invention according to the concentration of sulfuric acid were examined and the results are shown in Table 3 and FIG.
6 is a graph showing a removal rate according to sulfuric acid concentration in a process for producing high purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention.
As shown in Table 3 and FIG. 6, the removal rate of Li was 52% when the solution was removed from the 2 M solution of sulfuric acid, the removal rate of Ni was 89%, and the removal rate of Na was 87% Was able to separate more than 50% by 2M stripping solution. In addition, the removal rate of organic phase increased with increasing sulfuric acid concentration, but the removal rate did not increase with sulfuric acid concentration exceeding 6M.
Experimental Example 4: Analysis of nickel, lithium and sodium content in nickel sulfate
The content of nickel, lithium and sodium in the nickel sulfate crystallized in the cooling process in the process for producing high purity nickel sulfate from the cobalt extraction residue of the lithium secondary battery according to the present invention was analyzed.
It was found that the high-purity nickel sulfate of 99.99% can be produced because the amount of Na and Li is extremely small at 24.6 ppm of Li and 154 ppm of Na in the nickel sulfate produced by the production method of the present invention.
Although a specific embodiment of a method for producing high purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery according to the present invention has been described above, it is apparent that various modifications are possible within the scope of the present invention.
Therefore, the scope of the present invention should not be limited to the above-described embodiments, but should be determined by the scope of the appended claims and equivalents thereof.
It is to be understood that the foregoing embodiments are illustrative and not restrictive in all respects and that the scope of the present invention is indicated by the appended claims rather than the foregoing description, It is intended that all changes and modifications derived from the equivalent concept be included within the scope of the present invention.
Claims (10)
Mixing the nickel-extracted organic phase with a 6M sulfuric acid removing agent to remove Ni, Li and Na at 100% and concentrating the nickel with nickel sulfate; And
Heating the concentrated nickel sulfate to 70 to 90 DEG C and then cooling to crystallize the nickel sulfate;
Wherein the basic solution is mixed at a volume ratio of 0.1 to 0.2 with respect to the extractant to saponify the extractant at 60 vol%.
The extractant may be selected from the group consisting of di-2-ethylhexylphosphoric acid (D2EHPA), 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester : PC88A), a mixture of di-2-ethylhexylphosphoric acid and tri-butyl-phosphate (TBP) and a mixture of 2-ethylhexylphosphonic acid mono-2- Wherein the lithium secondary battery is one selected from the group consisting of a mixture of 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester and tri-butyl-phosphate (TBP) Purity nickel sulfate from the extraction residue.
Wherein the basic solution is NaOH or NH 4 OH. 2. The process according to claim 1, wherein the basic solution is NaOH or NH 4 OH.
Wherein the ratio of the organic phase to the aqueous phase (O / A) in the mixture of the extraction residue remaining after extracting the cobalt with the extractant and the basic solution is 1.
Wherein the extraction step is carried out four times. The method for producing high purity nickel sulfate from a cobalt extraction residue of a lithium secondary battery.
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Cited By (3)
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WO2018070690A1 (en) * | 2016-10-10 | 2018-04-19 | 재단법인 포항산업과학연구원 | Method for increasing concentration of metal salt, and method and apparatus for recovering metal salt crystal from metal salt solution |
CN109777954A (en) * | 2019-03-13 | 2019-05-21 | 荆门市格林美新材料有限公司 | A kind of extracting method of mine liquid intermediate ion |
KR20190074416A (en) | 2017-12-20 | 2019-06-28 | 주식회사 포스코 | Method for manufacturing high purity metal salt |
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KR20190074416A (en) | 2017-12-20 | 2019-06-28 | 주식회사 포스코 | Method for manufacturing high purity metal salt |
CN109777954A (en) * | 2019-03-13 | 2019-05-21 | 荆门市格林美新材料有限公司 | A kind of extracting method of mine liquid intermediate ion |
CN109777954B (en) * | 2019-03-13 | 2021-01-05 | 荆门市格林美新材料有限公司 | Method for extracting ions in mineral liquid |
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